CN101180099B - Alkyl sulfate free and orthophosphate free dentifrice composition comprising a fluoride source and a silica dental abrasive - Google Patents
Alkyl sulfate free and orthophosphate free dentifrice composition comprising a fluoride source and a silica dental abrasive Download PDFInfo
- Publication number
- CN101180099B CN101180099B CN200680017226.6A CN200680017226A CN101180099B CN 101180099 B CN101180099 B CN 101180099B CN 200680017226 A CN200680017226 A CN 200680017226A CN 101180099 B CN101180099 B CN 101180099B
- Authority
- CN
- China
- Prior art keywords
- compositions
- toothpaste
- fluoride
- composition
- enamel
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Landscapes
- Cosmetics (AREA)
Abstract
A dentifrice composition is described for combating dental erosion and/or tooth wear comprising a fluoride ion source and a silica dental abrasive, the dentifrice having a Relative Dentine Abrasivity (RDA) value from 20 to 60 and a pH in the range 6.5 to 7.5 and being free of an orthophosphate buffer or a water soluble salt of a C10-18 alkyl sulfate.
Description
The present invention relates to resist the oral care composition of (namely prevent, suppress and/or treat) dental erosion and/or odontotripsis.
Dental calculus is mainly by calcium hydroxy apetite Ca
10(PO
4)
6(OH)
2Form, calcium hydroxy apetite can part be replaced by anion (for example carbanion or fluorion) and cation (for example zinc ion and magnesium ion).Dental calculus also contains non-apatite mineral phase, for example OCP and calcium carbonate.
Dental caries can cause occuring tooth loss, and it is a kind of multi-factor disease, wherein Production by Bacteria acid, and for example lactic acid finally forms cavity so that lower surface demineraliting (and incomplete remineralization) causes carrying out sex organization's forfeiture.The biomembranous existence of bacterial plaque is essential condition, and when easy fermenting carbohydrate, for example sucrose level continues a period of time of rising, and acidogenic bactria for example Streptococcus mutans (S.mutans) becomes pathogenic bacterium.
Even without ill, acid attack and/or physical abrasion can cause occuring dental hard tissue's forfeiture; Believe now that these processes are collaborative and carry out.Dental hard tissue is exposed to and causes demineraliting in the acid, causes surperficial softening, mineral density reduction.Under normal physiological conditions, the demineraliting tissue carries out self-regeneration by the remineralization effect of saliva.Saliva is oversaturated to calcium and phosphoric acid, and the Healthy People purpose that salivates is the flush away acid attack, and heightening pH makes mineral deposition to change balance.
Dental erosion is a kind of superficial phenomenon that comprises demineraliting, finally causes dental surface dissolving (caused by acid, do not derive from antibacterial).Acid the most generally derives from diet, for example from the citric acid of fruit or soda pop, from the phosphoric acid of cola drink and from the acetic acid of aromatic vinegar juice.Repeatedly contact the hydrochloric acid (HCl) that is produced by stomach and also can cause dental erosion, for example gastroesophageal reflux or the induced reaction that suffers by the bulimia nerovsa patient enter the oral cavity to this hydrochloric acid by natural reaction.
Odontotripsis is caused by abrasion and/or friction.When rubbing each other, dental surface wears away, i.e. the Two body wear form.An obvious example of usually observing among the crowd is exactly bruxism, i.e. a kind of custom of grinding one's teeth in sleep, and its active force is large, take accelerated wear test as feature, particularly on occlusal surface.Three-body-abrasion usually causes rubbing, and modal example is to brush teeth relevant with using toothpaste.Commercial toothpastes has been down to minimum to the caused abrasion levels of the enamel that mineralizes fully, seldom or do not have a clinical consequences.Yet if enamel is exposed under the erosion environment demineraliting, softening, enamel will become more responsive to odontotripsis.Dentin is softer than enamel, and is therefore more responsive to wearing and tearing.The people that dentin exposes should avoid the toothpaste that uses abrasivus content high, and for example those are based on the toothpaste of aluminum.Moreover, because the softening tissue that will increase of corrosional dentin is to the sensitivity of wearing and tearing.
Dentin is very important tissue, is usually covered by enamel or cementum in vivo according to its position, and it is the same to root of the tooth namely to refer to respectively corona.It is higher that dentin and enamel are compared the content of organic matter, and its architectural feature is to exist the tubule that is full of fluid, and this tubule is flowed through to odontoblast/dental pulp contact surface from dentin-enamel surface or dentin-cementum joint.The cause of extensively generally acknowledging dental hypersensitiveness relates to fluid flow variations (fluid dynamic theory) in the exposure tubule, causes being considered to be positioned near the mechanoreceptor of odontoblast/dental pulp contact surface and is upset.The dentin of not all exposure all is responsive because dentin usually coated (interlock mixture) cover, the interlock mixture mainly comprises mineral and the protein that derives from dentin self, but also contains the organic component that derives from saliva.Along with passage of time, the tissue that mineralizes that little tube chamber piles with is more and more.Form the dentin of reparation in order to adapt to dental pulp wound or chemical stimulation, this point is also well proved.But erosion can be removed coating and tubule " filler ", causes that the dentin fluid outwards flows, so that dentin stimulates (for example heat, cold-peace pressure) more responsive to external world.As previously mentioned, corroding also can be so that dentin surface be more responsive to wearing and tearing.In addition, increase along with exposing the tubule diameter, the dental hypersensitiveness aggravation, and because the tubule diameter increases towards odontoblast/dental pulp contact surface direction, so the dentin abrasion that constantly increases progressively can cause anaphylaxis to rise, particularly in the situation of dentin Fast Wearing.
Erosion and/or acid mediated wearing and tearing cause the forfeiture of protectiveness adamantine layer, expose following dentin, therefore are that the Etiological that dental hypersensitiveness occurs is learned factor.
Now advocate the increase that acid is absorbed to diet and reduce the rising that the dinner number of times is followed dental erosion and odontotripsis sickness rate.In view of this, will be conducive to help oral care composition prevention dental erosion and odontotripsis.
Oral care composition usually contains the promotion remineralization of teeth and strengthens the acid proof fluoride sources of dental hard tissue.In order to produce curative effect, dental hard tissue's picked-up that fluorion must just received treatment.Yet some composition of toothpaste for example abrasive silicas can disturb picked-up, thereby has reduced the intake of free available fluorion.
A way that addresses this problem in United States Patent (USP) 4340583 (Huber) advise that this patent has been described a kind of dentifrice composition, it comprises fluoride sources, is equipped with the abrasive silicas that has excellent compatibility through special processing and fluorion.The pH of this compositions in the 4-8 scope, preferred 6.5-7.5, and contain soluble phosphate pellicle penetrating agent, preferred example is orthophosphate.Embodiment 11 has described a kind of toothpaste with low-friction agent level, and this toothpaste contains the alkyl sodium sulfate as surfactant.
Another solution is advised in WO01/66074 (Colgate), this patent recommendation fluoride source should be stored under the alkaline pH (to be avoided interacting with abrasive silicas, this effect can occur under acid pH), but in order to improve enamel to the picked-up of fluorion, should under acid pH, absorb fluorion.This can be by realizing with biphase composition toothpaste, and one mutually for alkalescence and contain fluorion, and another for acid and contain phosphate anion, mixes both mutually before use, and a kind of phosphate fluoride composition (pH 4-6) of acid is provided.
WO 04/012693 (Colgate) has described a kind of dentifrice composition, its desensitization and tooth Fluoridation and remineralization effect are improved, its invigoration effect obviously can combine to realize with potassium salt by fluorion, the pH of said composition and cushions with alkali metal phosphate in the 7.5-9 scope.
The invention provides a kind of dentifrice composition that resists more prevalent dental erosion and/or odontotripsis problem, said composition comprises fluoride sources and silica for toothpaste abrasive agent, the relative dentin abrasion of toothpaste (Relative Dentine Abrasivity, RDA) value is 20-60, pH and does not contain orthophosphate buffer agent or water solublity C in the 6.5-7.5 scope
10-18Alkyl sulfate.
The pH that relates to refers to as dentifrice composition water measured pH during by weight ratio homogenate in 1: 3.
Compositions of the present invention is useful especially for anti-dental erosion, thereby because they not only can reinforce the tooth opposing acid attack that takes care of one's teeth, and can reinforce again the softening enamel that is caused by acid attack.
In addition, because the low wear intensity of the present composition, neutral pH and do not contain the C that is usually used in oral cavity composition in fact
10-18The strong surfactant of alkyl sulfate (for example sodium lauryl sulfate) is so compositions of the present invention can't make the problem relevant with dental erosion and odontotripsis be worsened.
Therefore, the advantage that compositions of the present invention has effective remineralization and reinforces tooth, thus take care of one's teeth opposing dental erosion and/or odontotripsis and treatment dental erosion and/or odontotripsis are provided.
Compositions of the present invention also can be used for prevention and treatment dental caries and/or dental hypersensitivity.
The suitable fluorine ion source that uses in the present composition comprises alkali metal fluoride (for example sodium fluoride), alkali metal mono-fluor phosphate (for example sodium monofluorophosphate), stannous fluoride or amine fluoride, the fluorion amount that provides is 25-3500pm, preferred 100-1500ppm.Preferred fluoride source is sodium fluoride, for example prescription can contain 0.1-0.5% weight, for example the sodium fluoride of 0.205% weight (equaling the fluorion of 927ppm), 0.2542% weight (equaling the fluorion of 11 50ppm) or 0.315% weight (equaling the fluorion of 1426ppm).
The suitable present composition does not comprise the calcium salt that can reduce free fluorion utilization rate.
The example of suitable silica for toothpaste abrasive agent comprises on the market Zeodent, Sident, Sorbosil or the Tixosil (trade name) of Huber, Degussa, Ineos and each self-sales of Rhodia company.Abrasive silicas answers capacity to have to guarantee that the RDA of toothpaste is between 20-60, preferably between 25-50, more preferably between 25-40, when guaranteeing the suitable cleaning teeth of toothpaste, do not encourage tooth wear, the tooth that particularly suffers dental erosion or caused by acid attack softening.
Usually, abrasive silicas accounts at most 15% of total composition weight, the 2-10% of total composition weight for example, preferably at least 5%, 5-7% for example, particularly 6%.Reduce the horizontal advantage of abrasive silicas and be, not only reduced the wear intensity of toothpaste, and it is minimum that the interaction of abrasivus and fluorion is down to, thereby improved the utilization rate of free fluorion.
The suitable surfactant of using among the present invention comprises amphoteric surfactant, long-chain alkyl lycine for example, for example Albright﹠amp on the market; ' EmpigenBB ' (trade name) that Wilson company sells; preferred chain alkyl amido alkyl betaine; cocamido propyl betaine for example; or low ionic surface active agent; sodium methylcocoyltaurate for example; be the Adinol CT (trade name) that Croda company sells, perhaps their mixture.
Amphoteric surfactant can be used as single surfactant and uses separately or can use together in conjunction with low ionic surface active agent.
The content of suitable surfactant is the 0.1-10% of total composition weight, preferred 0.1-5%, more preferably 0.5-1.5%.
The pH of dentifrice composition is in the 6.5-7 scope, and suitable pH is 6.8-7.2, for example 7.1, can add alkali for example sodium hydroxide regulate pH.Avoid by contrast adding the orthophosphate buffer agent with the instruction of above-mentioned Colgate house journal application, because the existence of orthophosphate buffer salt can reduce enamel to the picked-up of fluoride.
In order to treat dental hypersensitivity, suitable dentifrice composition of the present invention also comprises the desensitizer of desensitization.The example of desensitizer comprises tubule blocker or neural desensitizer and their mixture, for example desensitizer described in the WO 02/15809 (Block).Preferred desensitizer comprises strontium salt for example strontium chloride, strontium acetate or strontium nitrate, or potassium salt for example potassium citrate, potassium chloride, potassium bicarbonate, potassium gluconate, particularly potassium nitrate.
The potassium salt of desensitization is generally the 2-8% of total composition weight, for example can use the potassium nitrate that accounts for total composition weight 5%.
Having of potassium nitrate is beneficial to the clean effect that enhancing is provided, and this prescription for low frictional properties is particularly useful, otherwise can think that the prescription of low frictional properties has relatively low clean-up performance.
With many previous disclosed composition for desensitizing that contain potassium salt (for example EP 278744 (Unilever), WO 93/2514 (Procter﹠amp; Gamble) and EP 1040819 (Pfizer) with, compositions of the present invention does not contain sodium lauryl sulfate, because sodium lauryl sulfate when having good decontamination and clean-up performance, can cause forming insoluble lauryl potassium sulfate precipitate.
Compositions of the present invention also can comprise anti-erosion agent, for example WO 04/054529 (Procter﹠amp; Gamble) polymeric mineral surface active agent described in.
In order to reach described purpose, compositions of the present invention will contain proper formulation agent (formuating agent), for example thickening agent, wetting agent, aromatic, sweeting agent, opacifier or coloring agent, antiseptic and water all are selected from conventional those formula agents that use in the oral hygiene composition field.
Suitable thickening agent comprises for example non-ionic thickening agent, for example (C1-6) alkyl cellulose ether, for example methylcellulose; Hydroxyl (C1-6) alkyl cellulose ether, for example hydroxyethyl-cellulose and hydroxypropyl cellulose; (C2-6) (C1-6) alkyl cellulose ether of alkylene oxide modification, for example hydroxypropyl emthylcellulose; And their mixture.Also can use other thickening agent, for example the material of natural gum and rubber polymer or similar glue, for example Irish gum (Irish Moss), Xanthan gum, gum tragacanth, sodium carboxymethyl cellulose, polyvinylpyrrolidone, starch and thickening property silicon dioxide.Thickening agent is preferably the mixture of thickening property silicon dioxide and Xanthan gum.
Suitable amount of thickener is the 0.1-30% of total composition weight, preferred 1-20%, more preferably 5-15%.
The suitable wetting agent that uses in the present composition comprises for example glycerol, xylitol, sorbitol, propylene glycol or Polyethylene Glycol or their mixture; Wetting agent content is the 10-80% of total composition weight, preferred 20-60%, more preferably 25-50%.
Preferred opacifier is titanium dioxide, and its content is the 0.05-2% of total composition weight, preferred 0.075-0.2%, for example 0.1%.This content has improved the visual appearance effect of compositions.
Suitable relative amount composition can be mixed to prepare compositions of the present invention, this point is easily, and after this if necessary, scalable pH obtains final desirable value.
The present invention also provides a kind of anti-dental erosion and/or odontotripsis method, and the method comprises the present composition of the individuality that needs are arranged being used effective dose.Described compositions is also to the prevention of dental caries and/or dental hypersensitivity with treat useful (if particularly it also contains aforesaid desensitizer).
Further specify the present invention by the following example.
Can estimate the fluoride utilization rate, enamel of toothpaste of the present invention to picked-up, acid protection effect, wear intensity and the cleaning capacity of fluoride with following method.
The picked-up of embodiment 4-fluoride and acid protection
The fluoride utilization rate of present embodiment is described the present composition (seeing Table 1) that has been research and comparison and commercially available toothpaste with fluoride, enamel are to picked-up and the acid protection effect (using remineralization/demineraliting circulating research to estimate) of fluoride.
The research of fluoride utilization rate
1 part of test toothpaste was prepared sample in 10 minutes with the homogenize of 3 parts of (w/w) distilled water.Measure the pH of serosity, in about 10, the centrifugal acquisition supernatant of 000rpm.The dilute with water supernatant is so that fluorinion concentration is in the working standard scope.Adopt inhibition type electric conductance to detect Dionex
The chromatography of ions is analyzed this solution.By external standard method Measurement and analysis substrate concentration.
Fluoride utilization rate and the pH of various test products have been listed in the Table I.These containing sodium fluoride toothpaste all demonstrate good fluoride utilization rate.
Table I-available fluoride and pH
Enamel is to the picked-up (EFU) of fluoride
Carry out the EFU test operation according to the operation 40 described in U.S. food Drug Administration (FDA) test operation.In the case, use the 0.1M lactic acid (pH5.0 adds hydroxyapatite to 50% saturation) that contains 0.2%w/v polyacrylic acid (carbopol 907) to form initial damage.
Select people's incisor healthy, top, the center, wash all adhesion soft tissues.Prepare the enamel axle that diameter is 3mm with every tooth of hollow diamond bit perpendicular cuts to labial surface.Can finish under water this process in order to prevent that sample is overheated.Use methylmethacrylate each sample packages to be imbedded the end (1/4 " diameter * 2 " are long) of lucite bar.Cut away too much acrylic acid, enamel surface is come out.The enamel sample wets/dried paper polishing with 600 granularities, then again with ultra-fine γ-type aluminium oxide polishing.
Then, each enamel sample is immersed 0.5ml 1M perchloric acid (HClO
4) in 15 seconds, and do not stop to stir, the enamel sample is etched.Then regulate buffer (TISAB-Orion Research Inc. with the total ionic strength adjustment buffer degree, Cambridge, MA) every kind of sample solution being buffered to pH is 5.2 (0.25ml samples, 0.5ml TISAB and 0.25ml 1N sodium hydroxide), determine content of fluoride (1ml standard substance and 1mlTISAB) by the standard curve that contrasts same preparation.These data have reflected the front intrinsic fluoride level of each sample process.
Sample is repeatedly ground as previously mentioned and polishes.At room temperature, each enamel sample was immersed in 0.1M lactic acid/0.2% carbopol, 907 solution 24 hours, form initial damage.Then fully clean these samples with distilled water, it is stored under the wet environment until use.
Sample immersed in the 25ml supernatant (the centrifugal acquisition of serosity that corresponding 1 part of toothpaste is formed after with the homogenize of 3 parts of (w/w) distilled water) process continuous stirring (350rpm) 30 minutes.After in deionized water, cleaning, use foregoing 15 seconds 1M HClO
4Corrode and remove surface layer, measure content of fluoride.Then with fluoride number after each sample process deduct process before the variation that draws content of fluoride in the enamel of fluoride (intrinsic) level, with it owing to test processes.Carry out statistical analysis with the one-way analysis of variance model.When showing significant difference, adopt multipole poor method of inspection (Student Newman-Keuls (SNK) test) to analyze individual average.
Table II has been listed the toothpaste of embodiment 2 and the EFU result of study of multiple commercial toothpastes.Although all prescriptions all have identical fluoride source and similar fluoride utilization rate, in tested product, the toothpaste of the embodiment of the invention 2 demonstrates outstanding EFU statistically.
Table II-external fluoride picked-up research
*The standard error of average (n=12) ± average
Judge that with multipole poor method of inspection the value (using different letter representations) that draws has significant difference (p＜0.05).
External remineralization/demineraliting research
The purpose of this research is that simulation is exposed under the dynamical state of diet acid, estimates toothpaste with fluoride and promotes enamel to the picked-up of fluoride and the effect that reduces follow-up demineralized.Select 1%w/v citric acid monohydrate acidic buffer (transferring pH to 3.8 with NaOH), conform to total titrable acidity with the pH of orange juice.
According to the described method of front EFU prepare embedding the enamel sample (the 3mm diameter, n=18).They are used as healthy sample or slightly corrode sample.Use Vickers micro hardness tester (load 200g stopped 15 seconds) to measure surface microhardness (SMH).Impression everywhere on each sample surface is measured average sample hardness, with Vickers hardness number (VNH) expression.
Place the 5.0ml citrate buffer solution to stir in each sample and estimated adamantine acid resistance in 11 minutes.Then sample is immersed and left standstill again in the 10ml citrate buffer solution 20 minutes.And then measure SMH, will be divided into several groups by aching and limpization sample according to the SMH after corroding.With people's saliva of mixing and 50: 50 mixture containing mucinous artificial saliva buffer (M-ASB) as the remineralization medium in all cyclic tests.M-ASB comprises 2.20g/l gastric mucin, 0.381g/l sodium chloride, 0.213g/l dewater calcium chloride, 0.738g/l KH2PO4 and 1.114g/l potassium chloride.At least collect people's saliva that wax stimulates with it from five people, mixing, freezing until use.Then vigorous stirring is mixed saliva sample, saliva sample (7.5ml saliva+7.5ml M-ASB) is assigned to 30ml process beaker.Use fresh saliva/mineral mixed liquor every day.
During processing, sample is immersed daily the brushing teeth of simulation in the toothpaste serosity.5.0g toothpaste is added in the fresh saliva of 10g in the beaker/mineral mixed solution, uses the magnetic stirrer prepared slarry.Before each the processing, just prepare fresh serosity.Day round-robin method comprises 5 * 2 minutes acid attack phases and 3 * 2 minutes processing phases.After the processing, clean sample with the distilled water that flows, then use saliva/M-ASB to replace and process sample.Measured again SMH after circulating in 10 days and 20 days.The treatment schedule that is used for this test is as follows:
A.8:00-8:02 toothpaste processes 1
*
B.8:02-10:00 saliva is processed
C.10:00-10:02 acidic buffer corrodes 1
D.10:02-11:00 saliva is processed
E.11:00-11:02 acidic buffer corrodes 2
F.11:02-12:00 saliva is processed
G.12:00-12:02 toothpaste processes 2
H.12:02-13:00 saliva is processed
I.13:00-13:02 acidic buffer corrodes 3
J.13:02-14:00 saliva is processed
K.14:00-14:02 acidic buffer corrodes 4
L.14:02-15:00 saliva is processed
M.15:00-15:02 acidic buffer corrodes 5
N.15:02-16:30 saliva is processed
O.16:30-16:32 toothpaste processes 3
P.16:32-8:00 saliva is processed
Q. return (a)
*First day, this processes omission; Before any processing, in saliva, begin test after 1 hour to allow to form pellicle.
After processing scheme finished in 20 days, use the content of fluoride of each enamel sample of micro-drilling technology to 100 μ m depth survey.Calculate the fluoride data as fluoride weight (the μ g F/cm of per unit sample
3).
Carry out statistical analysis with the one-way analysis of variance model.When showing significant difference, adopt multipole poor method of inspection (SNK) to analyze individual average.
Table III has been listed described result of study.
SMH and fluoride picked-up in Table III-following remineralization/demineralization
*The standard error of average (n=18) ± average
Judge that with multipole poor method of inspection the value (using different letter representations) that draws has significant difference (p＜0.05) in the intermediate hurdles.
SMH microhardness (VHN) data show 10 days and 20 days the time, the relatively not contrast of fluoride, and the toothpaste of embodiment 2 and Crest mothproof toothpaste are preventing that acid mediated enamel sample has significant difference statistically aspect softening.Yet when 10 days and 20 days, the toothpaste of embodiment 2 demonstrates more outstanding protective effect (Table III) statistically than Crest mothproof toothpaste.In addition, during studying, the SMH that the toothpaste of embodiment 2 is compared damage also embodies net increase.The toothpaste of fluoride picked-up data show embodiment 2 is compared with the Crest mothproof toothpaste and more can be promoted the fluoride picked-up.Increasing to some extent aspect the fluoride picked-up although observe the Crest mothproof toothpaste on the numeral, the contrast of fluoride not there is no significant difference relatively.
Described research not only proved the protection enamel resist more multi-surface softening aspect, the toothpaste of embodiment 2 is better than the Crest mothproof toothpaste statistically, and describedly studies show that specifically the enamel of damage can be reinforced again.The acid degree of protection becomes positive correlation with the fluoride degree that sample absorbs, this show more effectively absorb fluoride from the toothpaste of embodiment 2 can be so that sour demineraliting be resisted in protection is improved and promotes more effective remineralization.
In short, described in vitro study has proved that compositions of the present invention provides outstanding level of protection in the repeatedly damage that anti-diet acid attack causes.
The external sclerous tissues of embodiment 5-abrasion research
Radioactive dentin and enamel abrasion research carry out according to previous report document (Hefferen, J.Dent.Res.55 563-573,1976 and Hefferen etc., J.Dent.Res.63 1176-1179,1984).
Dentin or enamel sample are placed neutron flux, so that controlled generation radioactivity in the sample
32P.Then, sample packages is embedded in the methylmethacrylate, in order to they are fixed in the horizontal Tooth-brushing device of V-8.Use brush teeth essential sample 1500 times of serosity (containing 10g pyrophosphoric acid dicalcium in 50ml 0.5% carboxymethyl cellulose (CMC) glycerite), enamel 5000 times is as pretreatment.Also serosity is used as intrinsic reference standard.The toothbrush that uses is specified as ADA (ADA), load 150g.
After the pretreatment, the toothbrush of applied load 150g is brushed teeth essential 1500 times in such as the serosity of sandwich sample design, perhaps enamel is tested for 5000 times, and wherein every kind of test material serosity (25g toothpaste adds 40ml water) is clipped in the middle by reference material serosity (10g/50ml 0.5%CMC).The water contrast only comprises 50ml water.When occuring when brushing teeth, the particle of enamel or dentin surface is ground in serosity for toothbrushing.Whole minute serosity diluted with scintillating medium, use scintillation counter to measure radioactivity, namely lose in the sample
32P.
Then calculate reference material to the front and back net value of every kind of test serosity, averaging.Test serosity average is used for calculating RDA or REA to the ratio of reference average.The test serosity obtains the RDA value to the ratio multiplication by constants 100 of reference serosity, multiply by 10 and obtains the REA value.
RDA and REA result that the external wear test of the toothpaste of embodiment 2 and multiple commercial toothpastes obtains have been listed respectively in Table IV and the Table V.In tested toothpaste, the toothpaste of embodiment 2 demonstrates minimum RDA and REA, shows the wearing and tearing of low-down sclerous tissues.
Table IV-external relative dentin abrasion research
*The standard error of average (n=8) ± average
Table V-external relative enamel abrasion research
*The standard error of average (n=8) ± average
The external microhardness research of embodiment 6-
This embodiment describes is further to studies show that the compositions of the present invention enamel of can reinforcing and harden, and can resist for the protection of tooth danger and treatment dental erosion and the odontotripsis of dental erosion and odontotripsis.
Citric acid monohydrate, magnesium chloride, calcium chloride dihydrate, potassium chloride, ammonium chloride, N-2-hydroxyethyl piperazine-N '-ethyl sulfonic acid (HEPES), sodium hydroxide and potassium hydroxide are all available from Sigma-Aldrich (Dorset, UK).KH2PO4 is available from VWR (Poole, UK).The Stycast acrylic resin is available from Hitek Electronic Materials (Scunthorpe, UK).The artificial saliva of using composed as follows: magnesium chloride (0.20mM), calcium chloride dihydrate (1.0mM), KH2PO4 (4.0mM), HEPES (20.0mM), potassium chloride (16.0mM), ammonium chloride (4.5mM).Regulate pH to 7.0 with potassium hydroxide (1.0M).
Test formulations as shown in Table VI.
The detailed prescription of tested toothpaste in Table VI-microhardness research.Prescription pH (weight ratio) mastic deionized water serosity (MFP: sodium monofluorophosphate, AmF: amine fluoride, NaF: sodium fluoride, SLS: sodium lauryl sulphate) that relates to 1: 3.
Statistical analysis
Data are carried out variance analysis, relatively the difference between individual the processing.Significant difference is set as p＜0.05.Use soft SA S (combination process) analytical data (SAS software study institute, Kai Rui, the U.S.).
The preparation of healthy enamel sample
The people who extracts ground one's teeth in sleep and after premolars removes root of the tooth and dental pulp, be kept in the saturated thymol aqueous solution.Before the use, thoroughly clean tooth, check the damage sign.Use Buddha's warrior attendant saw (Struers Minitom) to downcut healthy enamel section from the cheek-tongue side face of tooth.Section is embedded in the acrylic resin to process spends the night.Then, use the silicon carbide paper of 1200 and 2400 granularities to polish sample, 4 ℃ of storing and dryings.Before using sample was placed deionized water rehydration at least 60 minutes.
Microhardness
Use Struers Duramin-1 microsclerometry instrument (meeting Vickers Buddha's warrior attendant durometer) to measure sample SMH.Sample load 1.961N (200g) stopped 20 seconds.With Vickers hardness number (VHN) expression SMH, the sample VHN of each time point is based on the average of six hardness numbers.
The enamel surface of citric acid mediation is softening
Measure the SMH of 24 healthy enamel samples as baseline, and be 4 processed group (n=6) with the sample random assortment.Measure respectively the SMH numerical value of each sample, as its automatic control contrast.The sample immersion is spent the middle stirring of the standby toothpaste serosity (1: 3) of ion water making 120 seconds.Then use the washed with de-ionized water sample, immersed the middle total of 1% citric acid (pH3.75) 30 minutes.Sample was taken out in 10 minutes in every interval, after remaining acid is removed in cleaning in deionized water, measured SMH.
Shown in Fig. 1 is the softening result of study of enamel surface.Now the relative baseline of SMH value is done standardization.At all time points, relatively use the sample of the control treatment of Colgate-Palmolive anti-anaphylaxis toothpaste and non-fluoride, process the softening sample in the surface that is caused by acid with toothpaste and the Elmex anti-anaphylaxis toothpaste of embodiment 1, its softening degree presents remarkable reduction statistically.After 20 minutes and 30 minutes, the toothpaste of embodiment 1 is compared with Elmex anti-anaphylaxis toothpaste, and it suppresses acid mediated surperficial softening degree and is better than statistically Elmex anti-anaphylaxis toothpaste, but is not after 10 minutes.At 20 minutes and 30 minutes point, Colgate-Palmolive anti-anaphylaxis toothpaste was compared with the contrast of fluoride not, and it suppresses surperficial softening degree and is better than statistically the not contrast of fluoride, but is not at 10 minutes.
Fig. 1. use before the independent pretreatment of mastic deionized water serosity in 1: 3 impact for enamel SMH in 2 minutes being exposed to 1.0% citric acid (pH3.75)
Summarize, the softening model of enamel surface has proved that now compositions of the present invention can protect the enamel opposing to corrode, and therefore can be used for providing protection opposing dental erosion and odontotripsis.
Reharden after the damage
Respectively 24 healthy enamel samples are immersed 30 minutes preparation erosion damages in the 10 ml1.0%w/w citric acid solutions (pH3.75).Then measure SMH as baseline, the sample random assortment is become 4 processed group (n=6).In addition, measure respectively the SMH value of each sample, as its automatic control contrast.The sample immersion is spent the middle stirring of the standby toothpaste serosity (1: 3) of ion water making 120 seconds.Then use the washed with de-ionized water sample, be placed on to absorb in the analogue body in the artificial saliva that contains whole minute corresponding dentifrice slurry liquid and fill a prescription.
Carry out three researchs that separate with the initial mastic prescription simulation of high dilution gradually with the absorption strength that exists in several minutes and a few hours salivas behind the toothpaste.The initial selection with the mastic (research R1) of artificial saliva by dilution in 1: 1426.This dilution so that in the saliva fluoride concentration be about 1ppm.In ensuing test, increase the dilution level so that the fluoride final concentration is about 0.04ppm and about 0.02ppm (being respectively research R2 and R3) in the artificial saliva.Measure the degree of rehardening of sample after in the artificial saliva of improvement, hatching 4 hours, 24 hours and 48 hours.Fig. 2-4 summarized respectively enamel reharden research R1-R3 result's (comprising commercial toothpastes).Again the relative baseline of SMH value is done standardization.
Fig. 2. rehardening of enamel erosion damages: after 2 minutes, then in the artificial saliva of the relevant toothpaste improvement with whole minute, hatch and generate the fluoride that final concentration is about 1ppm with mastic deionized water serosity processing in 1: 3
In research R1, when artificial saliva contains when having an appointment the 1ppm fluoride, at all time points, all processed group are compared with baseline, and its degree of rehardening has significant difference statistically.At 4 hours, all its degree of rehardening of processing based on fluoride were better than the not contrast of fluoride statistically; At this time point, on numeral between the Fluoridizing group, do not demonstrate significant difference statistically.Yet at 24 hours and 48 little time points, its degree of rehardening of the toothpaste processed group of embodiment 1 was better than all other processed group statistically.At 24 hours and 48 hours, Elmex anti-anaphylaxis toothpaste obviously was better than the contrast of Colgate-Palmolive anti-anaphylaxis toothpaste and non-fluoride.At 48 hours, Colgate-Palmolive anti-anaphylaxis toothpaste was better than the not contrast of fluoride statistically, but was not at 24 hours.
Fig. 3 and Fig. 4 have summarized respectively the data of research R2 and R3.Viewed similar among block diagram trend and Fig. 2.
Fig. 3. rehardening of enamel erosion damages: after 2 minutes, then in the artificial saliva of the relevant toothpaste improvement with whole minute, hatch and generate the fluoride that final concentration is about 0.04ppm with mastic deionized water serosity processing in 1: 3
In addition, all processed group are compared with baseline, and the erosion damages of rehardening presents significant difference statistically.At all time points, its degree of rehardening of the toothpaste processed group of embodiment 1 is better than the contrast of Colgate-Palmolive anti-anaphylaxis toothpaste and non-fluoride statistically, at 24 hours and 48 little time points, is better than statistically Elmex anti-anaphylaxis toothpaste.At 4 hours, do not observe significant difference between the contrast of Elmex anti-anaphylaxis toothpaste, Colgate-Palmolive anti-anaphylaxis toothpaste and non-fluoride, yet at 24 hours and 48 little time points, Elmex anti-anaphylaxis toothpaste was better than the contrast of Colgate-Palmolive anti-anaphylaxis toothpaste and non-fluoride statistically.Point at any time, Colgate-Palmolive anti-anaphylaxis toothpaste is not better than the not contrast of fluoride statistically.
Fig. 4. rehardening of enamel erosion damages: after 2 minutes, then in the artificial saliva of the relevant toothpaste improvement with whole minute, hatch and generate the fluoride that final concentration is about 0.02ppm with mastic deionized water serosity processing in 1: 3
Video data has clearly illustrated that the erosion damages of can rehardening among Fig. 2-4, and uses toothpaste with fluoride can promote to reharden.The rising of now believing enamel SMH shows injury repairing has occured that new mineral deposition is in the lower surface of enamel surface and demineraliting during this period.
Toothpaste and Elmex anti-anaphylaxis toothpaste with embodiment 1 are processed erosion damages, the relatively not contrast of fluoride, these two kinds of toothpastes with fluoride are put at any time the degree of rehardening and are all presented statistically significant difference, and in all three researchs, except R3, not remarkable 4 hours difference.At 24 hours and 48 little time points, and process comparing of observing with Elmex anti-anaphylaxis toothpaste, process with the toothpaste of embodiment 1 and cause all the time damaging stronger rehardening.Therefore, this trend does not rely on the fluoride level that is added in the artificial saliva in research range.Injury repairing speed is also to the horizontal relative insensitivity of the fluoride in the artificial saliva.This will show that initial treatment is key factor, and it has determined the follow-up degree of rehardening.Process damage and process comparing of observing with the contrast toothpaste of fluoride not with Colgate-Palmolive anti-anaphylaxis toothpaste, cause the orientation reinforcement of rehardening.In this case, free fluoride level will be very low during serosity is processed, yet in artificial saliva between incubation period, MFP has an opportunity to be combined with enamel surface to be hydrolyzed.In research R1, the complete hydrolysis of the MFP that exists in artificial saliva will expect to generate at least free fluoride of 1ppm.
Summarize, microhardness research has now demonstrated the enamel surface that toothpaste with fluoride can suppress to be caused by citric acid softens, and can promote again the reparation of enamel erosion damages.Specifically, the toothpaste of the embodiment 1 that uses in this research, this toothpaste is designed to enamel to be strengthened high-caliber available fluoride picked-up, and the prospect that fully shows aspect enamel protection and injury repairing is long-range.
Embodiment 7-decontamination effect
This embodiment has described two kinds of diverse ways, is used for compositions more of the present invention and several commercial toothpastes (Elmex
Sensitive (Gaba, Switzerland), SensodyneMultiCare
With Aquafresh Fresh ' n ' Minty
) detergency ability.
Pellicle cleaning ratio method
PCR uses the baurodont enamel of incision, polishing and acid attack as substrate, makes up and manually catches the complex that mixes diet chromogen and chromogenic bacteria.All PCR test is pressed described in the Stookey etc. (J.Dent.Res.61:1236-1239,1982) and is carried out.
Table VII has provided toothpaste and the Elmex of the embodiment 1 that measures
The PCR value of toothpaste.
The toothpaste of Table VII-embodiment 1 and Elmex
The PCR value of Sensitive toothpaste
| Product | The PCR value (standard error of mean value ± average, n=16) |
| The toothpaste of embodiment 1 | 46±4 |
Elmex
 |
52±5 |
With regard to cleaning capacity, do not have significant difference statistically between the described value.
Intrinsic exogenous decontamination (NESR) method
Cut cattle front tooth hat, removal dental pulp, cleaning and dry in deionized water.100g spontaneous recovery acrylic acid repair materials powder and 40 g spontaneous recovery liquid acrylics (all available from Bracon Ltd.) are mixed with acrylic acid embedding liquid.Pouring the mixture that obtains into diameter is that 3.5 centimetres, height are in 1.5 centimetres the bottle cap (Ecotrin, Van Blarcom Closures).Each lid between hardening period pushes tooth to be guaranteed in the mixture with the surface near level.All teeth are embedded in lid central authorities.
Use Ou Le B40 indication toothbrush to place the 42-rank to move back and forth the machining groove of Tooth-brushing device the tooth of embedding, so that toothbrush moves back and forth up and down between tooth.In toothbrush load 100g situation, brush speed is 100 circulations of per minute.
With 1 of Macleans Milkteeth and deionized water: the 3w/w serosity is brushed teeth 10 minutes to remove unstable spot.Take out tooth, in water, clean, then air dried overnight.
Use Hunterlab Huntercolour LS6100 tintometer and CIE laboratory L
*A
*B
*L in the grade
*Spot on the parameter evaluation tooth.Choose every tooth per five flat position point readings all around.After each processed group is brushed teeth at random in advance, the L of tooth
*The value scope is 50-90.
Relative datum contrast (B) comes the detergency ability of evaluation test toothpaste (A).In order to compare two products (A is to B), tooth is divided into two groups at random.The processing stage of the first step, brush first group of tooth 30 minutes with the 1+1w/w serosity of prescription A and deionized water, brush second group of tooth with prescription B under the similarity condition.The same cleaning and dry tooth.Record L
*Value is the processing stage that then tooth entering second step.In this stage, process the previous group of processing with prescription A with prescription B, process the previous group of processing with prescription B with prescription A.The same cleaning, dry tooth are measured L
*Value.Each processed group comprises 14 teeth, and namely per two kinds of products are relatively used 28 teeth.
By in each processing sequence relatively the first step processing stage during total spot number of removing divided by two steps processing stage of decontamination stain number estimate the relative decontamination effect of A and B.That is to say, whether Δ L
*(T1[A])/Δ L
*(T1[A])+Δ L
*(T2[B]) and Δ L
*(T1[B])/Δ L
*(T1[B])+Δ L
*(T2[A]) has significant difference (P＜0.05, two tail t checks) statistically, the processing stage that wherein T1 and T2 representing respectively 1 and 2, A and B represent respectively prescription A and B.Be worth with percentage ratio herein and represent, be limited in the 0-100% scope.
The toothpaste that lower Table VIII has provided embodiment 1 respectively with Sensodyne MultiCare
, Aquafresh Fresh ' n ' Minty
And Elmex
The compare NESR value of gained of Sensitive toothpaste.
The toothpaste of Table VIII-embodiment 1 is to the NESR value of commercially available prod
Table VIII demonstrates in the NESR model, and its dirt-removing power of the toothpaste of embodiment 1 is better than Sensodyne MultiCare
Or Aquafresh Fresh ' n ' Minty
Toothpaste.Although do not have significant difference in 5% level, the toothpaste that data also provide some information to show embodiment 1 can surpass Elmex
Sensitive toothpaste (but for the first time decontamination 42% of Tooth paste brush of usefulness embodiment 1, and use Elmex
But for the first time decontamination 32% of Tooth paste brush).
For a kind of product with low wear intensity, the detergency ability of the toothpaste of embodiment 1 is high.Part reason is to have this performance and it seems it is owing to there is 5%KNO in prescription
3May be owing to exist the lime nitrate of relative high dissolubility to cause this effect to raise, that is to say that because the existence of nitrate ion, some calcium in the spot are discharged in the solution, thereby have weakened spot substrate.
Claims (13)
1. the dentifrice composition of an anti-dental erosion; said composition comprises: the sodium fluoride that exists as the amount so that the 25-3500ppm fluorion to be provided of fluoride sources; as the amphoteric surfactant that accounts for compositions 0.1-10% weight of surfactant or be the low ionic surface active agent of sodium methylcocoyltaurate or their mixture; with the silicon dioxide toothpaste abrasives that accounts at most compositions 15% weight as abrasivus; the relative dentin abrasion value of toothpaste is 20-60; pH does not contain orthophosphate buffer agent or water solublity C10-18 alkyl sulfate or calcium salt in the scope of 6.5-7.5.
2. the compositions of claim 1, wherein the abrasivus capacity exists to guarantee that the relative dentin abrasion value of toothpaste is 25-50.
3. the compositions of claim 2, wherein the relative dentin abrasion value of toothpaste is 25-40.
4. wherein there are simultaneously amphoteric surfactant in claim 1 or 2 compositions and are the low ionic surface active agent of sodium methylcocoyltaurate.
5. claim 1 or 2 compositions, wherein amphoteric surfactant exists as single surfactant.
6. claim 1 or 2 compositions, wherein amphoteric surfactant is the chain alkyl amido alkyl betaine as cocamido propyl betaine.
7. claim 1 or 2 compositions, wherein pH is in the scope of 6.8-7.2.
8. claim 1 or 2 compositions, said composition also comprises desensitizer.
9. the compositions of claim 8, wherein desensitizer is potassium salt, is selected from potassium nitrate, potassium citrate, potassium chloride, potassium bicarbonate, potassium gluconate or their mixture.
10. the compositions of claim 8, wherein desensitizer is potassium nitrate.
11. the compositions of claim 1 or 2, said composition also comprise anti-erosion agent.
12. the compositions of claim 1 or 2, said composition also comprise the titanium dioxide as opacifier, its content is the 0.05-2% of total composition weight.
13. the purposes of the compositions of claim 1 or 2 in the medicine of the anti-dental erosion of preparation and/or odontotripsis.
Applications Claiming Priority (5)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| GB0505760.9 | 2005-03-21 | ||
| GB0505760A GB0505760D0 (en) | 2005-03-21 | 2005-03-21 | Novel composition |
| GB0525458.6 | 2005-12-14 | ||
| GB0525458A GB0525458D0 (en) | 2005-12-14 | 2005-12-14 | Novel composition |
| PCT/EP2006/002665 WO2006100071A1 (en) | 2005-03-21 | 2006-03-17 | Alkyl sulfate free and orthophosphate free dentifrice compostion comprising a fluoride source and a silica dental abrasive |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101180099A CN101180099A (en) | 2008-05-14 |
| CN101180099B true CN101180099B (en) | 2013-02-06 |
Family
ID=34531591
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN200680017226.6A Active CN101180099B (en) | 2005-03-21 | 2006-03-17 | Alkyl sulfate free and orthophosphate free dentifrice composition comprising a fluoride source and a silica dental abrasive |
Country Status (3)
| Country | Link |
|---|---|
| CN (1) | CN101180099B (en) |
| GB (1) | GB0505760D0 (en) |
| ZA (1) | ZA200708069B (en) |
Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB0822434D0 (en) * | 2008-12-09 | 2009-01-14 | Glaxo Group Ltd | Novel use |
| CN101829032B (en) * | 2010-05-11 | 2013-02-13 | 李少君 | Dual-purpose toothpaste composition and preparation method thereof |
| US11202736B2 (en) | 2018-02-15 | 2021-12-21 | Imam Abdulrahman Bin Faisal University | Antimicrobial dental restoratives containing coconut oil and/or derivatives of coconut oil |
| CN108618980A (en) * | 2018-06-08 | 2018-10-09 | 叶绿芝生物科技（中山）有限公司 | A kind of multi-functional liquid tooth paste |
| CN109662931A (en) * | 2019-03-01 | 2019-04-23 | 中山市怡口康科技有限公司 | Children oral essence |
| CN109846780A (en) * | 2019-03-06 | 2019-06-07 | 叶绿芝生物科技（中山）有限公司 | A kind of liquid tooth paste |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5045305A (en) * | 1986-10-02 | 1991-09-03 | Chesebrough-Pond's Usa Co., Division Of Conopco, Inc. | Oral hygiene composition |
| US5993784A (en) * | 1997-07-24 | 1999-11-30 | Whitehill Oral Technologies | Low foaming therapeutic toothpastes with improved cleaning and abrasion performance |
-
2005
- 2005-03-21 GB GB0505760A patent/GB0505760D0/en not_active Ceased
-
2006
- 2006-03-17 CN CN200680017226.6A patent/CN101180099B/en active Active
-
2007
- 2007-09-19 ZA ZA200708069A patent/ZA200708069B/en unknown
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5045305A (en) * | 1986-10-02 | 1991-09-03 | Chesebrough-Pond's Usa Co., Division Of Conopco, Inc. | Oral hygiene composition |
| US5993784A (en) * | 1997-07-24 | 1999-11-30 | Whitehill Oral Technologies | Low foaming therapeutic toothpastes with improved cleaning and abrasion performance |
Also Published As
| Publication number | Publication date |
|---|---|
| ZA200708069B (en) | 2009-01-28 |
| GB0505760D0 (en) | 2005-04-27 |
| CN101180099A (en) | 2008-05-14 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| EP1868689B1 (en) | Alkyl sulfate free and orthophosphate free dentifrice composition comprising a fluoride source and a silica dental abrasive | |
| Imfeld | Prevention of progression of dental erosion by professional and individual prophylactic measures | |
| Stookey et al. | The relative anticaries effectiveness of three fluoride-containing dentifrices in Puerto Rico | |
| Bajaj et al. | Comparison of CPP-ACP, tri-calcium phosphate and hydroxyapatite on remineralization of artificial caries like lesions on primary enamel-An in vitro study | |
| CN101180099B (en) | Alkyl sulfate free and orthophosphate free dentifrice composition comprising a fluoride source and a silica dental abrasive | |
| MX2008012908A (en) | Oral care regimens and kits. | |
| CN108618980A (en) | A kind of multi-functional liquid tooth paste | |
| CN101677918A (en) | Novel use | |
| US8623333B2 (en) | Composition | |
| Reich et al. | Mouthrinses and dental caries | |
| RU2553365C2 (en) | Oral care composition applicable for dental erosion and/or wear control | |
| AU2008265190A1 (en) | Mouthwash composition comprising xanthan gum and sodium fluoride | |
| JP2021529794A (en) | Toothpaste containing carboxylic acid or alkali metal salt thereof and a source of free fluoride ions | |
| Nalini et al. | Remineralizing Potential of Various Commercially Available Dentifrices on Artificial Enamel Lesions | |
| US10143633B2 (en) | Treating cariogenic diseased oral biofilm with elevated pH | |
| RU2816006C2 (en) | Dentifrice composition containing carboxylic acid or its alkali metal salt and source of free fluoride ions | |
| CN109846780A (en) | A kind of liquid tooth paste | |
| Alnujaym et al. | ASSESSMENT OF FLUORIDE UPTAKE BY TOOTH ENAMEL FROM DIFFERENT FLUORIDE DENTIFRICES | |
| JP2021529795A (en) | Toothpaste containing PVM-MA copolymer and source of free fluoride ions |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20210104 Address after: Meade Sykes Patentee after: GlaxoSmithKline Consumer Healthcare (UK) IP Ltd. Address before: British Ahmed Sykes Patentee before: GLAXO Group Ltd. |